Water → Ethyl 1-(3-cyano-4-hydroxyphenyl)pyrazole-4-carboxylate

HRID 850065노트

반응식

HRID 850065 반응식
[C:1]([C:3]1[CH:4]=[C:5]([N:11]2[CH:15]=[C:14]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH:13]=[N:12]2)[CH:6]=[CH:7][C:8]=1[O:9]C)#[N:2].[Cl-].[Al+3].[Cl-].[Cl-].O>ClC(Cl)C>[C:1]([C:3]1[CH:4]=[C:5]([N:11]2[CH:15]=[C:14]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH:13]=[N:12]2)[CH:6]=[CH:7][C:8]=1[OH:9])#[N:2]

참가 물질

5

반응물 3

HCID 962WaterHCID 6451240Aluminum(III) ChlorideHCID 19366041Ethyl 1-(3-cyano-4-methoxyphenyl)pyrazole-4-carboxylate

생성물 1

HCID 15407383Ethyl 1-(3-cyano-4-hydroxyphenyl)pyrazole-4-carboxylate수율 84.7%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

반응 조건

온도
70 °C

실험 절차

To a solution (280 ml) of ethyl 1-(3-cyano-4-methoxyphenyl)pyrazole-4-carboxylate (28 g) in dichloroethane was added aluminum chloride (47.6 g with stirring, and the mixture was heated at 70° C. for 4 hours. After the completion of the reaction, the reaction mixture was poured into water, extracted with ethyl acetate, washed with water and dried over magnesium sulfate. The solvent was evaporated under reduced pressure and the obtained residue was recrystallized from ethyl acetate to give 22.5 g of ethyl 1-(3-cyano-4-hydroxyphenyl)pyrazole-4-carboxylate, melting point 233-234° C. ##STR19##

후처리

  1. customAfter the completion of the reaction
  2. extractionextracted with ethyl acetate
  3. washwashed with water
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe obtained residue was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-a4eebd45252244e5891ad6b4c86300ff
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06015829

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